CN102324505B - Preparation method of graphene loaded with anatase type nano titanium dioxide and application thereof - Google Patents
Preparation method of graphene loaded with anatase type nano titanium dioxide and application thereof Download PDFInfo
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- CN102324505B CN102324505B CN201110211177.2A CN201110211177A CN102324505B CN 102324505 B CN102324505 B CN 102324505B CN 201110211177 A CN201110211177 A CN 201110211177A CN 102324505 B CN102324505 B CN 102324505B
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Abstract
The invention discloses a preparation method of graphene loaded with anatase type nano titanium dioxide and an application thereof. The preparation method comprises the following steps: preparing graphite oxide from crystalline flake graphite; carrying out reduction reaction on the graphite oxide to obtain graphene by taking hydrazine hydrate as a reducing agent and sodium dodecyl benzene sulfonate as a dispersing agent; preparing titanium hydroxide colloidal solution by taking tetrabutyl titanate as a titanium source; mixing the ethanol solution of graphene and the titanium hydroxide colloidal solution, stirring and calcining to prepare the graphene loaded with anatase type nano titanium dioxide. The graphene loaded with anatase type nano titanium dioxide prepared by the method can be mixed with copper powder to prepare the negative electrode of a nickel-hydride secondary battery. The method provided by the invention has the advantages of simple preparation process and low cost and is easy to operate. When the prepared graphene loaded with anatase type nano titanium dioxide is used as the active material of the cathode of the secondary battery, the effects of high discharge specific capacity and good circulation stability are achieved.
Description
Technical field
The present invention relates to a kind of preparation method and application thereof of Graphene of load anatase titanium dioxide, belong to field of electrochemical power source.
Background technology
Graphene is the Two-dimensional Carbon atomic crystal of in recent years finding, is a kind of single or multiple lift graphite material as thin as a wafer, and it is one of the study hotspot in current carbonaceous material and Condensed Matter Physics field.Graphene is to construct zero dimension fullerene, one dimension carbon nano-tube, said three-dimensional body phase graphite Sp
2the basic system unit of hydridization carbon.Graphene has a lot of peculiar character.Graphene is a kind of material that there is no energy gap, shows metallicity; In the Graphene of individual layer, each carbon atom has a not electronics of Cheng Jian, therefore has extraordinary conductivity; Hole and electronics in Graphene are separated from each other, and have caused the generation of new electrical conductivity phenomenon, for example irregular quantum hall effect.Graphene has boundless application prospect, its peculiar character provides good Physical Experiment platform still to manufacture nano electron device---high frequency transistor and but the optimal material of electron transistor is also having very wide application prospect aspect micro-filter screen and superconduction.In addition, Graphene also shows good electro-chemical activity, is the energy storage material of excellent performance, as the negative material of Ni-MH battery, has huge application space.
Titanium dioxide is a kind of high yield, low cost, eco-friendly material; In charge discharge process, titanium dioxide can keep stable structure, and anatase-type nanometer titanium dioxide has good photocatalytic effect.Due to nanostructure and conductive coating effect, titanium dioxide is with a wide range of applications in large-scale energy storage research.
Related documents report [Self-Assembled TiO2-Graphene Hybrid Nanostructures for Enhanced Li-Ion Insertion], adopt self-assembling method to prepare the graphene composite material of nano titanium oxide load, research for lithium ion battery efficiency, the Graphene adopting in the document is rapid intensification expansion gained, gained graphene suspension poor stability, be unfavorable for that nano titanium oxide is dispersed on graphene sheet layer, in order to reach the object of dispersion and to adopt anion sulfate acid surfactant to carry out stabilisation to the aqueous solution of Graphene, improved preparation cost, contaminated environment.
Summary of the invention
The object of the invention is to provide a kind of preparation method and application thereof of Graphene of load anatase-type nanometer titanium dioxide, described preparation method's process is simple, and the Graphene of made load anatase titanium dioxide has high electrochemistry capacitance as nickel-hydrogen secondary battery negative electrode material.
The present invention is achieved by the following technical solutions, and a kind of preparation method of Graphene of load anatase-type nanometer titanium dioxide is characterized in that comprising following process:
(1) prepare graphite oxide: the H by every gram of natural flake graphite by mass concentration 98%
2sO
4ratio for 30-40ml, joins H by natural flake graphite
2sO
4in, under stirring in ice-water bath, by the mass ratio of potassium permanganate and natural flake graphite, be 5: 1, then add KMnO
4, reaction 0.5-2h, then, mixture is transferred in the water-bath of temperature 30-40 ℃, continue to stir 30～60min, be warming up to again temperature 50-70 ℃, stir 0.5-2h, by every gram of natural flake graphite deionized water 80-120mL, hydrogen peroxide 10-20mL ratio by mass concentration 30%, under continuing to stir, add successively deionized water and hydrogen peroxide reaction 10-20min, product is through centrifugation, filter cake washs to sulfate radical-free ion with hydrochloric acid and the deionized water of mass concentration 2-10% successively, in vacuum drying chamber, in temperature 50-80 ℃ of dry 24-48h, obtain graphite oxide again,
(2) prepare Graphene: the graphite oxide of step (1) system is dispersed in to compound concentration 0.5-1mg/ml solution in deionized water, and the ultrasonic 2-5h that peels off, obtains graphene oxide solution; In graphene oxide solution, add neopelex, the quality of neopelex and the mass ratio of graphite oxide are 1: (1-3), to adding mass concentration in graphene oxide solution, be 85% hydrazine hydrate again, the volumetric usage of this hydrazine hydrate solution is by every gram of graphite oxide 1-10ml, after temperature 70-80 ℃ of water-bath backflow 24-48h, product with deionized water wash to pH be 7, the Graphene obtaining is joined in absolute ethyl alcohol, be made into the ethanolic solution that concentration is the Graphene of 0.5-1mg/ml;
(3) prepare titanium hydroxide colloidal solution: butyl titanate is splashed into in absolute ethyl alcohol, to be mixed with volumetric concentration be that the solution of 1-3% is end liquid, under agitation in end liquid, drip mixed liquor, the hydrochloric acid that described mixed liquor is 36.5% by mass concentration, absolute ethyl alcohol and deionized water are by volume measured and are respectively 3～4 times, 1.5～1.8 times and 1.5～1.8 times of butyl titanate volume and form, and after mixed liquor dropwises, obtain titanium hydroxide colloidal solution;
(4) the titanium hydroxide colloidal solution that the ethanolic solution of Graphene step (2) being made makes with step (3) is (10-50) by volume: 1 ratio is mixed, stir 30min-60min, after standing 12-24h in drying box in temperature 60 C-80 ℃ evaporate to dryness, after being ground, the powder obtaining puts into tube furnace, flow with 100ml/min passes into argon gas, in argon gas atmosphere, by the heating rate of 10 ℃/min, be warming up to 300 ℃-500 ℃ calcining 2h-3h of temperature, obtain the Graphene of load anatase-type nanometer titanium dioxide.
With the application of the Graphene of the prepared load anatase-type nanometer titanium dioxide of said method, the Graphene of this load anatase-type nanometer titanium dioxide mixes the negative pole of nickel-hydrogen secondary cell processed with copper powder.
The present invention has the following advantages: the preparation method of the Graphene of load anatase-type nanometer titanium dioxide of the present invention, and process is simple, and easy operating, and cost is low.The titanium dioxide granule size of load is little and be uniformly dispersed.Using the Graphene of prepared load anatase-type nanometer titanium dioxide as the active material of nickel-hydrogen secondary battery negative electrode, and specific discharge capacity is high, and good cycling stability.
Accompanying drawing explanation
Fig. 1 is the SEM photo of the embodiment of the present invention 1 prepared Graphene.
Fig. 2 is the TEM photo of the embodiment of the present invention 1 prepared Graphene.
Fig. 3 is the TEM photo of the Graphene of the prepared load anatase-type nanometer titanium dioxide of the embodiment of the present invention 1.
Fig. 4 is the XRD spectra of the Graphene of the load anatase-type nanometer titanium dioxide that makes of the inventive method.The XRD spectra of the Graphene of the load anatase-type nanometer titanium dioxide that wherein (a) prepared for method described in embodiment 1; (b) XRD spectra of the Graphene of the load anatase-type nanometer titanium dioxide of preparing for method described in embodiment 2; (c) XRD spectra of the Graphene of the load anatase-type nanometer titanium dioxide of preparing for method described in embodiment 3.
Fig. 5 is that the Graphene of the prepared load anatase-type nanometer titanium dioxide of the embodiment of the present invention 1 is as the charging and discharging curve of the nickel-hydrogen secondary cell of negative material.
Fig. 6 is that the Graphene of the prepared load anatase-type nanometer titanium dioxide of the embodiment of the present invention 1 is as the stable circulation linearity curve of the nickel-hydrogen secondary cell of negative material.
Embodiment
In the sulfuric acid that is 98% in 120ml mass concentration, add 3g natural flake graphite, mixture is slowly added to 15g potassium permanganate in the speed whipping process with 200rpm in ice-water bath; After ice bath 2h, mixture is transferred in 35 ℃ of water-baths of temperature, continued to stir 1h; Warming-in-water to 65 ℃ of temperature are stirred to 2h, stir simultaneously, slowly add 250ml deionized water, at gained mixed liquor, add again deionized water to 1400ml, then to add 30ml mass concentration be 30% hydrogen peroxide, reaction 20min.The watery hydrochloric acid that is 5% by mass concentration by products therefrom carries out centrifuge washing, and washing is extremely without SO
4 2-(use BaCl
2check), the washings obtaining is dry in temperature 60 C in vacuum drying chamber, obtains graphite oxide.
Get the 100mg graphite oxide that above-mentioned steps makes and be dispersed in 100ml deionized water, the ultrasonic 2h that peels off, obtaining concentration is the graphene oxide solution of 1mg/ml.In graphene oxide solution, add 100mg neopelex, adding 0.1ml mass concentration is 85% hydrazine hydrate again, reductase 12 4h refluxes mixed liquor at 80 ℃ of temperature, then with the washing of 500ml deionized water, obtain Graphene, gained Graphene is joined after the ethanolic solution that ultrasonic dispersion in 100ml absolute ethyl alcohol obtains Graphene stand-by.
1.5ml butyl titanate is splashed in 50ml absolute ethyl alcohol as end liquid, 5ml mass concentration is that the mixed liquor of 36.5% hydrochloric acid, 2.5ml absolute ethyl alcohol and 2.5ml deionized water is as titrating solution, at rotating speed, be under 300rpm stirs, titrating solution is slowly added drop-wise in end liquid, after dripping 20min, obtain titanium hydroxide colloidal solution, get gained titanium hydroxide colloidal solution 10ml, join in the 100ml ethanolic solution of graphene-containing of gained in above-mentioned steps, under 200rpm rotating speed, stir after 0.5h dry in temperature 60 C in drying box.After the product obtaining is pulverized, in tube furnace, with the flow of 100ml/min, pass into argon gas, under argon gas atmosphere protection, calcine 2h after being warming up to 500 ℃ of temperature with the heating rate of 10 ℃/min, obtain the Graphene of load nano-titanium dioxide.
After being mixed with 180mg copper powder, the Graphene composite powder of 20mg load anatase-type nanometer titanium dioxide adds in people's mould, one deck nickel foam is all housed up and down, after suppressing 5min with powder compressing machine under 400MPa pressure, take out, obtain columned cathode sheets, after welding lead, by there being the side epoxy resin sealing of solder joint, obtain work electrode.Using high power capacity sintered nickel electrode as to electrode, and Hg/HgO is reference electrode. electrolyte is 6molL
-1kOH solution.Adopt three-electrode system, carry out electrochemical hydrogen storage performance test under atmospheric pressure at room, charging and discharging currents is 20mA, and electric discharge stopping potential is 0V (VS.Hg/HgO), and 100 cycles circulate.The charging and discharging curve that Fig. 5 is the graphene-supported composite titania material that adopts the inventive method and make, discharge capacity reaches 1194.2mAh/g first, discharge and recharge 66 circulations after discharge capacity reach maximum, be 1982.5mAh/g.The cyclical stability figure that Fig. 6 is the graphene-supported composite titania material that adopts the inventive method and make, its good cycling stability as seen, after 100 circulations, specific discharge capacity is not less than 1600.4mAh/g.
Embodiment 2
The process of Graphene that the present embodiment is prepared load anatase-type nanometer titanium dioxide is identical with the process of embodiment 1, different: 500 ℃ of the temperature of calcining heat in embodiment 1 change 400 ℃ of temperature into, calcine 2h, obtain the Graphene of nano titanium oxide load.By the XRD spectra of the Graphene of the made nano titanium oxide load of the present embodiment, as shown in Fig. 4 (b), the anatase crystal of nano titanium oxide is lower than degree of crystallinity in embodiment 1 as seen from the figure.
Embodiment 3
The process of Graphene that the present embodiment is prepared load anatase-type nanometer titanium dioxide is identical with the process of embodiment 1, different: 500 ℃ of the temperature of calcining heat in embodiment 1 change 300 ℃ of temperature into, calcine 2h, obtain the Graphene of nano titanium oxide load.By the XRD spectra of the Graphene of the made nano titanium oxide load of the present embodiment, as shown in Fig. 4 (c), the anatase crystal of nano titanium oxide is lower than degree of crystallinity in embodiment 1 and embodiment 2 as seen from the figure.
Embodiment 4
The process of Graphene that the present embodiment is prepared load anatase-type nanometer titanium dioxide is identical with the process of embodiment 1, different: by 10ml, to change the titanium hydroxide colloidal solution adding in the 100ml ethanolic solution to graphene-containing into 5ml, finally make the Graphene of load nano-titanium dioxide.
Embodiment 5
The process of Graphene that the present embodiment is prepared load anatase-type nanometer titanium dioxide is identical with the process of embodiment 1, different: by 10ml, to change the titanium hydroxide colloidal solution adding in the 100ml ethanolic solution to graphene-containing into 3.3ml, finally make the Graphene of load nano-titanium dioxide.
Embodiment 6
The process of Graphene that the present embodiment is prepared load anatase-type nanometer titanium dioxide is identical with the process of embodiment 1, different: by 10ml, to change the titanium hydroxide colloidal solution adding in the 100ml ethanolic solution to graphene-containing into 2.5ml, finally make the Graphene of load nano-titanium dioxide.
Embodiment 7
The process of Graphene that the present embodiment is prepared load anatase-type nanometer titanium dioxide is identical with the process of embodiment 1, different: by 10ml, to change the titanium hydroxide colloidal solution adding in the 100ml ethanolic solution to graphene-containing into 2ml, finally make the Graphene of load nano-titanium dioxide.
Claims (2)
1. a preparation method for the Graphene of load anatase-type nanometer titanium dioxide, is characterized in that comprising following process:
(1) prepare graphite oxide: the H by every gram of natural flake graphite by mass concentration 98%
2sO
4ratio for 30-40ml, joins H by natural flake graphite
2sO
4in, under stirring in ice-water bath, by the mass ratio of potassium permanganate and natural flake graphite, be 5: 1, then add KMnO
4, reaction 0.5-2h, then, mixture is transferred in the water-bath of temperature 30-40 ℃, continue to stir 30～60min, be warming up to again 50-70 ℃, stir 0.5-2h, by every gram of natural flake graphite deionized water 80-120mL, hydrogen peroxide 10-20mL ratio by mass concentration 30%, under continuing to stir, add successively deionized water and hydrogen peroxide reaction 10-20min, product is through centrifugation, filter cake washs to sulfate radical-free ion with hydrochloric acid and the deionized water of mass concentration 2-10% successively, in vacuum drying chamber, in temperature 50-80 ℃ of dry 24-48h, obtain graphite oxide again,
(2) prepare Graphene: the graphite oxide of step (1) system is dispersed in to compound concentration 0.5-1mg/ml solution in deionized water, and the ultrasonic 2-5h that peels off, obtains graphene oxide solution; In graphene oxide solution, add neopelex, the quality of neopelex and the mass ratio of graphite oxide are 1: (1-3), to adding mass concentration in graphene oxide solution, be 85% hydrazine hydrate again, the volumetric usage of this hydrazine hydrate solution is by every gram of graphite oxide 1-10ml, after temperature 70-80 ℃ of water-bath backflow 24-48h, product with deionized water wash to pH be 7, the Graphene obtaining is joined in absolute ethyl alcohol, be made into the ethanolic solution that concentration is the Graphene of 0.5-1mg/ml;
(3) prepare titanium hydroxide colloidal solution: butyl titanate is splashed into in absolute ethyl alcohol, to be mixed with volumetric concentration be that the solution of 1-3% is end liquid, under agitation in end liquid, drip mixed liquor, the hydrochloric acid that described mixed liquor is 36.5% by mass concentration, absolute ethyl alcohol and deionized water are by volume measured and are respectively 3～4 times, 1.5～1.8 times and 1.5～1.8 times of butyl titanate volume and form, and after mixed liquor dropwises, obtain titanium hydroxide colloidal solution;
(4) the titanium hydroxide colloidal solution that the ethanolic solution of Graphene step (2) being made makes with step (3) is (10-50) by volume: 1 ratio is mixed, stir 30min-60min, after standing 12-24h in drying box in temperature 60 C-80 ℃ evaporate to dryness, after the powder obtaining is ground, in argon gas atmosphere, by the heating rate of 10 ℃/min, be warming up to 300 ℃-500 ℃ calcining 2h-3h, obtain the Graphene of load anatase-type nanometer titanium dioxide.
2. an application for the Graphene of the load anatase-type nanometer titanium dioxide making with method claimed in claim 1, the Graphene of this load anatase-type nanometer titanium dioxide mixes the negative pole of nickel-hydrogen secondary cell processed with copper powder.
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